CN101062031A - Method of controlling the quality of silymarin oral aolid preparation - Google Patents
Method of controlling the quality of silymarin oral aolid preparation Download PDFInfo
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Abstract
The invention discloses an oral solid preparation benefiting for liver with hepadestal as main component, which is characterized by the following: adopting high effective liquid phase method; checking the content of hepadestal; choosing alcohol solution or dilute hydrochloric acid solution as dissolving out medium; testing dissolving degree with ultraviolet spectrophoto method. This invention possesses strong exclusive property and high accuracy, accuracy rating and sensibility.
Description
Technical field
The present invention relates to the silymarin is that the silybin oral solid formulation of main component especially is the liver-benefiting dropping pill method of quality control of main component with the silymarin, it is characterized in that adopting high performance liquid chromatography to detect silymarin content, is that dissolution medium, ultraviolet spectrophotometry detect the silymarin dissolution with alcoholic solution or dilute hydrochloric acid solution.
Background technology
The Herba Silybi mariani prime system by the fruit of feverfew Silybum Herba Silybi mariani Silybum marianum (L) Gaertn through extracting the flavone compound of refining gained, main component is a silibinin, easily molten in dilute alkaline soln, be dissolved in acetone, in hot methanol, dissolve, slightly be dissolved in ethanol, slightly soluble in ethyl acetate, insoluble in water.The oral solid formulation that with the silymarin is main component has liver-benefiting dropping pill, Yiganling tablet, liver beneficial capsule, silybin granule, silybin ball etc., has the effect that improves liver function, protection liver plasma membrane, is used for acute and chronic hepatitis.
Because silymarin is water insoluble, so the important indicator of dissolution and content control becoming evaluation silymarin oral solid formulation formulation and technology and quality stability.But, having not yet to see the report of silymarin oral solid formulation dissolution detection method, assay mainly adopts ultraviolet spectrophotometry.
Summary of the invention
The invention provides that a kind of specificity is strong, accuracy and degree of accuracy and highly sensitive, content easy and simple to handle and dissolution detection method, for objective evaluation and effectively control with the silymarin be main component the silybin oral solid formulation especially the processing quality of liver-benefiting dropping pill foundation is provided.
For achieving the above object, the silybin oral solid formulation that the invention provides a kind of detection and with the silymarin be main component is silymarin content and quality control method for disolubility in the liver-benefiting dropping pill especially, and specific implementation method is as follows:
1. content assaying method: measure according to high performance liquid chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 D).
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; With methanol-water-0.5mol/L potassium dihydrogen phosphate (10: 10: 1) (regulating pH value to 4.0 with 0.2mol/L phosphoric acid) is mobile phase; The detection wavelength is 288nm.Number of theoretical plate calculates by the silibinin peak should be not less than 3000.
The preparation of reference substance solution is taken at 105 ℃ of silibinin reference substance 10mg that are dried to constant weight, and accurate the title decides, and puts in the 50ml measuring bottle, it is an amount of to add methanol, and supersound process (frequency is 40KHZ, and power is 120W) 20min makes dissolving, put coldly, be diluted to scale, shake up with methanol.Precision is measured 5ml, puts in the 25ml measuring bottle, is diluted to scale with mobile phase, shakes up, promptly.
The preparation sample thief of need testing solution an amount of (being equivalent to silymarin 24mg approximately), the accurate title, decide, and puts in the 100ml measuring bottle, it is an amount of to add methanol, supersound process (power is 120W, and frequency is 40KHZ) 20min makes dissolving, adds methanol and is diluted to scale, filter, the accurate subsequent filtrate of drawing, 5ml puts in the 25ml measuring bottle, adds mobile phase and is diluted to scale, shake up, promptly.
The algoscopy precision is drawn reference substance solution and each 20 μ l of need testing solution, injects chromatograph of liquid, measures in accordance with the law, presses external standard method with calculated by peak area, promptly.
2. dissolution detection method: sample thief according to dissolution method (two appendix XC of Chinese Pharmacopoeia version pharmacopeia in 2005), is a dissolution medium with dilute hydrochloric acid solution or alcoholic solution, and rotating speed is that per minute 50/100 changes, operation in accordance with the law.In the time of 30 minutes, get solution and filter, get subsequent filtrate as need testing solution.The about 10mg of silibinin reference substance that other learns from else's experience 105 ℃ and is dried to constant weight, the accurate title, decide, and puts in the 50ml measuring bottle, it is an amount of to add methanol, supersound process (frequency is 40KHZ, and power is 120W) 20min makes dissolving, puts cold, add methanol and be diluted to scale, shake up, the accurate 3ml that draws puts in the 50ml measuring bottle, adds dilute hydrochloric acid solution or alcoholic solution is diluted to scale, shake up, in contrast product solution.Get need testing solution and reference substance solution,, measure trap, calculate stripping quantity, promptly at 288nm wavelength place according to spectrophotography (appendix VA of Chinese Pharmacopoeia version in 2005).
The specific embodiment
Embodiment 1
High-efficient liquid phase technique is measured mobile phase, the mensuration wavelength of content and is selected and the system suitability test
Mobile phase is selected: with methanol: water: 0.5mol/L potassium dihydrogen phosphate (10: 10: 1) (regulating pH4.0 with 0.2mol/L phosphoric acid).
The mensuration wavelength is selected: the mobile phase solution of silibinin has absorption maximum at 288nm wavelength place.
The system suitability test: with octadecylsilane chemically bonded silica is filler, with methanol: water: 0.5mol/L potassium dihydrogen phosphate (10: 10: 1) (regulating pH4.0 with 0.2mol/L phosphoric acid) is a mobile phase, the detection wavelength is 288nm, and etection theory plate number is calculated as 5894 by silibinin.
Embodiment 2
High-efficient liquid phase technique is measured the linear test and the lowest detectable limit test of content
Linear test: get the about 10mg of silibinin reference substance, the accurate title, decide, and puts in the 50ml measuring bottle, and it is an amount of to add methanol, and supersound process (frequency is 40KHZ, and power is 120W) 20min makes dissolving, and is diluted to scale.The above-mentioned solution 3.0,4.0,5.0,6.0 of accurate absorption, 7.0ml put respectively in the 25ml measuring bottle, are diluted to scale with mobile phase, shake up, make the standard solution of series concentration, the accurate respectively 20 μ l that draw inject chromatograph of liquid, the record chromatogram the results are shown in Table 1.
Table 1. assay linear test result (n=5)
| Concentration (μ g/ml) | Peak area (A) |
| 0 24.41 32.54 40.68 48.82 56.95 | 0 663559 882449 1112665 1333878 1551942 |
With reference substance solution concentration is abscissa, and peak area is a vertical coordinate, calculates regression equation and gets: A=27300.52C-1405.57, r=0.9999.Show that concentration and chromatographic peak area are linear good in 24.41～56.95 μ g/ml scopes.
The lowest detectable limit test: when signal to noise ratio was 2: 1, minimal detectable concentration was 0.24 μ g/ml.
Embodiment 3
The stability test of high-efficient liquid phase technique assay solution
Concentration is the solution of 40 μ g/ml under the line taking test item, measures respectively at 0,2,4,6,8 hour under above-mentioned chromatographic condition, and mensuration solution is placed in 8 hours stable, the results are shown in Table 2.
Table 2. assay solution stability testing result
| Standing time (h) | Peak area (A) | Meansigma methods | RSD(％) |
| 0 2 4 6 8 | 1104940 1103343 1104454 1103909 1100304 | 1103390 | 0.17 |
Embodiment 4
The test of high-efficient liquid phase technique assay repeatability
It is a collection of to get liver-benefiting dropping pill, detects silymarin content according to method under the assay item, shows that the method repeatability is good, the results are shown in Table 3.
Table 3. assay repeatability test (n=6)
| (1) | (2) | (3) | (4) | (5) | X | RSD(％) | |
| Silibinin (peak area) | 1094786 | 1094711 | 1095326 | 1093452 | 1093583 | 1094372 | 0.07 |
Embodiment 5
The test of high-efficient liquid phase technique assay precision
Get 5 different times of a collection of branch of liver-benefiting dropping pill and repeat aforesaid operations, show that precision of method is good, the results are shown in Table 4.
Table 4. assay Precision test result (n=5)
| 1 | 2 | 3 | 4 | 5 | X | RSD(％) | |
| Silibinin content (mg) | 1.15 | 1.14 | 1.15 | 1.13 | 1.14 | 1.14 | 1.6 |
Embodiment 6
High-efficient liquid phase technique assay recovery test
Accurately take by weighing a certain amount of silibinin reference substance in the prescription ratio and mix,, carry out recovery test, show that the method accuracy is good, the results are shown in Table 5 according to the content assaying method operation with adjuvant.
Table 5. assay recovery test result
| Addition (mg) | The amount of recording (mg) | The response rate (%) | Average recovery rate (%) | RSD(％) |
| 8.14 10.17 12.20 | 8.17 8.17 8.17 10.08 10.08 10.09 12.17 12.15 12.17 | 100.37 100.37 100.37 99.12 99.12 99.21 99.75 99.59 99.75 | 99.7 | 0.5 |
Embodiment 7
High performance liquid chromatography detects silymarin content in the liver-benefiting dropping pill
Get three batches in liver-benefiting dropping pill sample, detect silymarin content, the results are shown in Table 6 according to content assaying method.
Table 6. liver-benefiting dropping pill assay result
| Sample | (1) | (2) | (3) |
| Silibinin content (mg/ ball) | 1.15 | 1.19 | 1.16 |
Embodiment 8
Dissolution detects the dissolution medium screening test
The reference substance solution preparation: the about 10mg of silibinin reference substance that learns from else's experience 105 ℃ and be dried to constant weight, the accurate title, decide, and puts in the 50mL measuring bottle, it is an amount of to add methanol, and supersound process (frequency is 40KHZ, and power is 120W) 20min makes dissolving, put cold, add methanol and be diluted to scale, shake up, the above-mentioned solution 3.0ml of accurate absorption, put in the 50ml measuring bottle, add 5% alcoholic solution and be diluted to scale, shake up, in contrast product solution (1).
The about 10mg of silibinin reference substance that learns from else's experience 105 ℃ and be dried to constant weight, the accurate title, decide, and puts in the 50mL measuring bottle, it is an amount of to add methanol, and supersound process (frequency is 40KHZ, and power is 120W) 20min makes dissolving, put cold, add methanol and be diluted to scale, shake up, the above-mentioned solution 3.0ml of accurate absorption, put in the 50ml measuring bottle, add the 0.1mol/L hydrochloric acid solution and be diluted to scale, shake up, in contrast product solution (2).
Test method and result: sample thief, according to dissolution method (two appendix XC of Chinese Pharmacopoeia version in 2005 three therapeutic methods of traditional Chinese medicine), be dissolution medium with 0.1mol/L hydrochloric acid solution, 5% alcoholic solution 250ml～400ml respectively, rotating speed is that per minute 50/100 changes, operation in the time of 15,30,45,60 minutes, is got solution 10ml respectively in accordance with the law, filter, get subsequent filtrate as need testing solution.
Get reference substance solution and need testing solution,, measure trap, calculate stripping quantity, the results are shown in Table 7 at the wavelength place of 288nm according to spectrophotography (appendix VA of Chinese Pharmacopoeia version in 2005).
Table 7. dissolution medium screening test result
Embodiment 9
Dissolution detects wavelength and selects test
Get silibinin reference substance 10mg, put in the 50ml measuring bottle, it is an amount of to add methanol, and supersound process (frequency is 40KHZ, and power is 120W) 20min makes dissolving,, add methanol to scale, shake up; Precision is measured 3ml, puts in the 50ml measuring bottle, adds 5% alcoholic solution and is diluted to scale, shake up, in the interscan of 200～400nm wave-length coverage, the result has absorption maximum at 288nm wavelength place according to spectrophotography (appendix VA of Chinese Pharmacopoeia version in 2005), so determine that detecting wavelength is 288nm.
Embodiment 10
Dissolution detects linear test
The about 5mg of silibinin reference substance that learns from else's experience 105 ℃ and be dried to constant weight, the accurate title, decide, put in the 50ml measuring bottle, add 10ml ethanol, (frequency is 40KHZ to supersound process, power is 120W) 20min makes dissolving, thin up is to scale, and precision is measured 0.5ml, 1.0ml, 2.0ml, 3.0ml, 4.0ml, 5.0ml, put respectively in the 25ml measuring bottle, add 5% alcoholic solution and be diluted to scale,, measure trap at 288nm wavelength place according to spectrophotography (appendix VA of Chinese Pharmacopoeia version in 2005), calculate regression equation and correlation coefficient, the results are shown in Table 8.
Table 8. dissolution detects linear result of the test
With the solution concentration is that abscissa, trap are vertical coordinate, carries out linear regression, and linear equation is: A=0.039c-0.0357, r=0.9999 show that concentration and trap are the good linear relation in 2.16 μ g/ml～21.04 μ g/ml scopes.
Embodiment 11
Dissolution detection assay solution stability testing
Getting above-mentioned concentration is 12 μ g/ml reference substance solution, measures trap according to said method respectively at 0,2,4,6,8 hour, shows that measuring solution stablized in 8 hours, the results are shown in Table 9.
Table 9. dissolution detects the solution stability testing result
| Standing time (h) | Trap (A) | A | RSD(％) |
| 0 2 4 6 8 | 0.4717 0.4721 0.4778 0.4799 0.4802 | 0.4763 | 0.78 |
Embodiment 12
The dissolution test method is selected test
The about 10mg of silibinin reference substance that the reference substance solution preparation is learnt from else's experience 105 ℃ and is dried to constant weight, the accurate title, decide, and puts in the 50ml measuring bottle, it is an amount of to add methanol, and supersound process (frequency is 40KHZ, and power is 120W) 20min makes dissolving, put cold, add methanol to scale, shake up, the accurate 3ml that draws, put in the 50ml measuring bottle, add 5% alcoholic solution and be diluted to scale, shake up, in contrast product solution.
The method sample thief, respectively according to dissolution method [Chinese Pharmacopoeia 2005 two appendix XC first methods of version (basket method) and second method (slurry method)], with 5% alcoholic solution is dissolution medium 400ml, rotating speed is that per minute 50/100 changes, in the time of 30 minutes, get solution, filter, get subsequent filtrate as need testing solution; Survey trap (A) at 288nm wavelength place according to spectrophotography (appendix VA of Chinese Pharmacopoeia version in 2005),
Calculate stripping quantity, the results are shown in Table 10.
Table 10. dissolution test method test result
| Dissolution rate (%) | ||
| The basket method | The slurry method | |
| 123456 meansigma methodss | 103.9 102.5 100.9 102.1 102.5 101.2 102.2 | 95.0 96.1 94.1 96.0 97.0 95.2 95.6 |
Embodiment 13
The dissolution detection method recovery test
Accurately take by weighing silibinin reference substance and adjuvant in the prescription ratio, mixing is made analog sample, measures silibinin content according to above-mentioned dissolution test method, carries out recovery test, shows that the method accuracy is good, the results are shown in Table 11.
Table 11. dissolution detection method recovery test result (n=9)
| Addition (mg) | The amount of recording (mg) | The response rate (%) | Average recovery rate (%) | RSD (％) |
| 7.89 10.62 12.38 | 7.81 7.67 7.73 10.61 10.47 10.45 12.42 12.41 12.37 | 99.0 97.2 98.0 100.0 98.6 98.4 100.3 100.2 99.9 | 99.1 | 1.1 |
Embodiment 14
The stripping uniformity test
Get liver-benefiting dropping pill, according to dissolution method (two appendix XC first methods of Chinese Pharmacopoeia version pharmacopeia in 2005), with 5% alcoholic solution 400ml is dissolution medium, rotating speed is that per minute 100 changes, operation in accordance with the law in the time of 2,5,10,20,30,45,60 minutes, is got solution 10ml (fluid infusion in time) respectively, filter, get subsequent filtrate as need testing solution; The about 10mg of silibinin reference substance that other learns from else's experience 105 ℃ and is dried to constant weight, the accurate title, decide, and puts in the 50mL measuring bottle, it is an amount of to add methanol, and supersound process (frequency is 40KHZ, and power is 120W) 20min makes dissolving, put cold, add methanol to scale, shake up, the accurate 3.0ml that draws, put in the 50ml measuring bottle, add 5% alcoholic solution and be diluted to scale, shake up, in contrast product solution.Get need testing solution and reference substance solution,, measure trap, calculate dissolution rate, show that the stripping homogeneity is good, the results are shown in Table 12 at 288nm wavelength place according to spectrophotography (appendix VA of Chinese Pharmacopoeia version in 2005).
Table 12. liver-benefiting dropping pill stripping uniformity test result
| Time (minute) | Dissolution rate (%) | Meansigma methods (%) | |||||
| 1 | 2 | 3 | 4 | 5 | 6 | ||
| 2 5 10 15 30 45 60 | 40.8 77.2 106.1 107.9 107.9 105.8 105.6 | 42.3 81.1 110.7 114.3 110.5 109.9 108.9 | 40.8 78.5 107.0 109.1 106.3 105.8 105.9 | 39.3 71.7 95.5 96.9 95.5 94.9 94.1 | 39.3 76.5 101.9 103.3 102.8 101.4 100.3 | 37.9 74.4 102.6 103.8 104.4 101.9 101.2 | 40.1 76.6 103.9 105.9 104.7 103.2 102.7 |
Embodiment 15
Dissolution test
Get three batches of liver-benefiting dropping pills and the above-mentioned dissolution test method of a collection of photograph of Yiganling tablet and carry out dissolution test, the results are shown in Table 13.
Table 13. liver-benefiting dropping pill and Yiganling tablet dissolution test result
| Time (minute) | Dissolution (%) | |||
| Liver-benefiting dropping pill | Yiganling tablet | |||
| (1) | (2) | (3) | (4) | |
| 2 5 10 15 30 45 60 | 40.1 76.6 103.9 105.9 104.7 103.2 102.7 | 39.3 75.7 99.5 98.9 96.2 92.9 98.2 | 37.9 73.6 100.2 99.3 97.9 93.3 98.1 | 2.2 5.1 7.2 10.2 20.0 25.2 32.2 |
Embodiment 16
Dissolution detects
Getting five batches of liver-benefiting dropping pills, according to dissolution determination (two appendix X of Chinese Pharmacopoeia version in 2005 C, first method), is dissolution medium with 5% alcoholic solution 400ml, rotating speed is that per minute 50/100 changes, and operation in accordance with the law is in the time of 30 minutes, get solution and filter, get subsequent filtrate as need testing solution; The about 10mg of silibinin reference substance that other learns from else's experience 105 ℃ and is dried to constant weight, the accurate title, decide, and puts in the 50ml measuring bottle, it is an amount of to add methanol, and supersound process (frequency is 40KHZ, and power is 120W) 20min makes dissolving, put cold, add methanol to scale, shake up, the accurate 3ml that draws, put in the 50ml measuring bottle, add 5% alcoholic solution and be diluted to scale, shake up, in contrast product solution.Get reference substance solution and need testing solution respectively,, measure trap, calculate the stripping quantity of every ball, the results are shown in Table 14 at 288nm wavelength place according to spectrophotography (appendix VA of Chinese Pharmacopoeia version in 2005).
Table 14. liver-benefiting dropping pill dissolution testing result
| Sample | (1) | (2) | (3) | (4) | (5) |
| Dissolution (%) | 98.1 | 105.9 | 98.3 | 103.9 | 99.7 |
Claims (3)
1. the silybin oral solid formulation that with the silymarin is main component especially is the liver-benefiting dropping pill method of quality control of main component with the silymarin, it is characterized in that it is to adopt high performance liquid chromatography to detect silymarin content, is that dissolution medium, ultraviolet spectrophotometry detect the silymarin method of dissolution with alcoholic solution or dilute hydrochloric acid solution.
2. claim 1 is described is that the silybin oral solid formulation of main component is the liver-benefiting dropping pill method of quality control of main component with the silymarin especially with the silymarin, it is characterized in that detecting according to an appendix VI of Chinese Pharmacopoeia version in 2005 D high performance liquid chromatography the method for silymarin content:
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; With methanol-water-0.5mol/L potassium dihydrogen phosphate (10: 10: 1) (regulating pH value to 4.0 with 0.2mol/L phosphoric acid) is mobile phase, and the detection wavelength is 288nm, and number of theoretical plate calculates by the silibinin peak should be not less than 3000;
The preparation of reference substance solution is taken at 105 ℃ of silibinin reference substance 10mg that are dried to constant weight, and accurate the title decides, and puts in the 50ml measuring bottle, it is an amount of to add methanol, and supersound process (frequency is 40KHZ, and power is 120W) 20min makes dissolving, put cold, be diluted to scale with methanol, shake up, precision is measured 5ml, put in the 25ml measuring bottle, be diluted to scale with mobile phase, shake up, promptly;
The preparation sample thief of need testing solution an amount of (being equivalent to silymarin 24mg approximately), the accurate title, decide, and puts in the 100ml measuring bottle, it is an amount of to add methanol, supersound process (power is 120W, and frequency is 40KHZ) 20min makes dissolving, adds methanol and is diluted to scale, filter, the accurate subsequent filtrate of drawing, 5ml puts in the 25ml measuring bottle, adds mobile phase and is diluted to scale, shake up, promptly;
The algoscopy precision is drawn reference substance solution and each 20 μ l of need testing solution, injects chromatograph of liquid, measures in accordance with the law, presses external standard method with calculated by peak area, promptly.
3. claim is described is that the silybin oral solid formulation of main component is the liver-benefiting dropping pill method of quality control of main component with the silymarin especially with the silymarin, it is characterized in that detecting the silymarin method of dissolution according to two appendix X of Chinese Pharmacopoeia version in 2005 C dissolution method:
Sample thief according to dissolution method (two appendix X of Chinese Pharmacopoeia version pharmacopeia in 2005 C), is a dissolution medium with dilute hydrochloric acid solution or alcoholic solution, and rotating speed is that per minute 50/100 changes, operation in accordance with the law; In the time of 30 minutes, get solution and filter, get subsequent filtrate as need testing solution; The about 10mg of silibinin reference substance that other learns from else's experience 105 ℃ and is dried to constant weight, the accurate title, decide, and puts in the 50ml measuring bottle, it is an amount of to add methanol, supersound process (frequency is 40KHZ, and power is 120W) 20min makes dissolving, puts cold, add methanol and be diluted to scale, shake up, the accurate 3ml that draws puts in the 50ml measuring bottle, adds dilute hydrochloric acid solution or alcoholic solution is diluted to scale, shake up, in contrast product solution; Get need testing solution and reference substance solution,, measure trap, calculate stripping quantity, promptly at 288nm wavelength place according to spectrophotography (an appendix V of Chinese Pharmacopoeia version in 2005 A).
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102478553A (en) * | 2010-11-23 | 2012-05-30 | 天津天士力制药股份有限公司 | Method for detecting silybin |
| CN113075370A (en) * | 2021-03-12 | 2021-07-06 | 药都(本溪)一致科技有限公司 | Method, system, medium and application for measuring quality consistency of traditional Chinese medicine |
| CN113340833A (en) * | 2021-05-31 | 2021-09-03 | 珠海天凯生物科技有限公司 | Dissolution rate detection method of tannic acid particles |
-
2007
- 2007-05-22 CN CN 200710106622 patent/CN101062031A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102478553A (en) * | 2010-11-23 | 2012-05-30 | 天津天士力制药股份有限公司 | Method for detecting silybin |
| CN113075370A (en) * | 2021-03-12 | 2021-07-06 | 药都(本溪)一致科技有限公司 | Method, system, medium and application for measuring quality consistency of traditional Chinese medicine |
| CN113340833A (en) * | 2021-05-31 | 2021-09-03 | 珠海天凯生物科技有限公司 | Dissolution rate detection method of tannic acid particles |
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